JP2000281523A - Cosmetic raw material, cosmetic and production of cosmetic - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a cosmetic composed of a cosmetic raw material capable of homogeneously dispersing a silicone oil or an organic oil and crosslinked silicone particles in a cosmetic and other cosmetic raw materials, containing the silicone oil or the organic oil and the crosslinked silicone particles in homogeneously dispersed state, giving good feeling to the finger and skin, having good spreadability and application feeling, effective for preventing the lifting hair, floating hair and entanglement and intertwining of hair to facilitate the bundling of hair and imparting the hair with dry feeling free from stickiness and provide a process for producing the cosmetic in high efficiency. SOLUTION: The objective cosmetic raw material is composed of an emulsion of a silicone oil or organic oil comprising droplets of a silicone oil or organic oil dispersed in water, having an average particle diameter of 0.1-500 μm and containing crosslinked silicone particles having an average particle diameter of 0.1-100 μm (the diameter of the crosslinked silicone particle is smaller than that of the silicone oil or organic oil droplet).

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a cosmetic raw material, a cosmetic, and a method for producing the cosmetic. More specifically, the present invention relates to a cosmetic raw material capable of uniformly dispersing silicone oil or organic oil and crosslinked silicone particles in cosmetic. Consisting of cosmetic ingredients and other cosmetic ingredients, it uniformly disperses silicone oil or organic oil and cross-linked silicone particles, has good touch, elongation, and feel on fingers and skin. The present invention relates to a cosmetic product that can prevent entanglement and entanglement, make it easier to tie hair, and give a dry feeling without stickiness, and a method for efficiently producing such a cosmetic product.

[0002]

2. Description of the Related Art Silicone oils, organic oils, silicone oils, organic oils, and the like are used as cosmetic raw materials for improving the feel and slipperiness of cosmetics on the skin and improving the feeling of use and slipperiness of hair cosmetics.
Alternatively, it is well known to mix crosslinked silicone particles, and it is also well known to mix silicone oil or organic oil in combination with crosslinked silicone particles. Examples of cosmetics containing silicone oil and crosslinked silicone particles include cosmetics containing crosslinked silicone particles having a three-dimensional network structure and high-viscosity or low-viscosity silicone oil (JP-A-1-165509, JP-A-1-165509).
1901577), cosmetics containing a crosslinked product of a hydrosilylation-crosslinking reactive silicone composition and a low-viscosity silicone oil (see JP-A-1-207354), crosslinked silicone, low-viscosity silicone oil, modified polyoxyalkylene silicone Cosmetic containing silicone oil emulsion consisting of water-based surfactant and water
(See Japanese Patent Application Laid-Open No. 3-79669), a base cosmetic containing a silicone oil emulsion of a low-viscosity silicone oil and a solid silicone at room temperature (Japanese Patent Application Laid-Open No. 3-27)
No. 1211), a skin cleansing agent containing silicone rubber and silicone oil (Japanese Patent Laid-Open No. 6-502).
646) and cosmetics comprising high molecular weight silicone and silicone rubber (see Japanese Patent Application Laid-Open No. 7-330537).

A hair cosmetic containing silicone oil and crosslinked silicone particles is disclosed in JP-A-2-172.
No. 906, Japanese Patent Application Laid-Open No. 5-139932 and Japanese Patent Application Laid-Open No. 10-36228 have been proposed. In particular, as hair cosmetics containing crosslinked silicone particles containing silicone oil, JP-A-2-243612
And JP-A-5-262987 have been proposed.

Further, cosmetics containing an organic oil and crosslinked silicone particles are disclosed in Japanese Patent Application Laid-Open No. 61-194509.
JP-A-63-313710, JP-A-7-31310
Japanese Patent Application Laid-Open No. 258027 and Japanese Patent Application Laid-Open No. 7-267820 have been proposed.

However, in these cosmetics, since silicone oil or organic oil and crosslinked silicone particles are blended with other cosmetic ingredients as cosmetic raw materials, the crosslinked silicone particles are not sufficiently dispersed in cosmetics, and the silicone oil or There is a problem that the compatibility between the organic oil and the crosslinked silicone particles is poor, and the original properties cannot be exhibited at all. In particular, in the case of water-based cosmetics, when dispersing silicone oil or organic oil and crosslinked silicone particles in other cosmetic raw materials, it is not possible to apply a sufficient shearing force. There was a problem that the feeling of use was bad.

[0006] Further, in hair cosmetics comprising silicone oil or organic oil and cross-linked silicone particles as cosmetic raw materials, the cross-linked silicone particles are not sufficiently dispersed in the hair cosmetic, and the silicone oil or organic oil is not used. The crosslinked silicone particles are poorly compatible,
There was a problem that the original characteristics could not be exhibited at all. In particular, in water-based hair cosmetics, when dispersing silicone oil or organic oil and crosslinked silicone particles in other hair cosmetic raw materials, it is not possible to apply a sufficient shearing force, and thus the stability of the hair cosmetic is not sufficient. And there is a problem that the feeling of use of hair cosmetics is poor.

[0007]

DISCLOSURE OF THE INVENTION The present inventors have intensively studied the above-mentioned problems, and as a result, have reached the present invention. That is, an object of the present invention is to provide a cosmetic raw material capable of uniformly dispersing silicone oil or organic oil and crosslinked silicone particles in cosmetics, comprising this cosmetic raw material and other cosmetic raw materials, and crosslinking with silicone oil or organic oil. Silicone particles are evenly dispersed, giving good feeling to fingers and skin, elongation, and feeling of use.Also, it prevents fuzzy hair, floating hair, tangles and entanglement, makes it easier to tie up hair, It is an object of the present invention to provide a cosmetic product capable of imparting a smooth feeling and a method for efficiently producing such a cosmetic product.

[0008]

Means for Solving the Problems The cosmetic raw material of the present invention comprises:
Droplets of silicone oil or organic oil having an average particle size of 0.1 to 500 μm dispersed in water are mixed with crosslinked silicone particles having an average particle size of 0.05 to 100 μm (however, the particle size of the crosslinked silicone particles is Or smaller than the particle size of the organic oil droplets). Further, the cosmetic raw material of the present invention is characterized by comprising an oil composition obtained by removing water from the above-mentioned emulsion and dispersing crosslinked silicone particles in silicone oil or organic oil. Further, the cosmetic of the present invention is characterized by comprising a cosmetic raw material comprising the above-mentioned emulsion and another cosmetic raw material. Also,
The cosmetic of the present invention is characterized by comprising a cosmetic raw material comprising the above oil composition and another cosmetic raw material. Furthermore, the method for producing a cosmetic of the present invention is characterized by blending the above-mentioned cosmetic raw material composed of the emulsion with another cosmetic raw material.

[0009]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS First, the cosmetic raw material of the present invention will be described in detail. The cosmetic raw material of the present invention is characterized by comprising a silicone oil or organic oil emulsion containing crosslinked silicone particles in droplets of silicone oil or organic oil dispersed in water. In this emulsion, the crosslinked silicone particles are used to crosslink the crosslinkable silicone composition. The crosslinkable silicone composition may be, for example, one obtained by a hydrosilylation crosslink reaction, one obtained by a condensation crosslink reaction, or one obtained by an organic peroxide crosslink. A reaction product and a product subjected to a high energy beam cross-linking reaction are mentioned. In particular, a product subjected to a hydrosilylation cross-linking reaction or a product subjected to a condensation cross-linking reaction is preferable.

In this emulsion, the type of the silicone oil is not limited, but those having a molecular structure such as linear, partially branched linear, cyclic, or branched are preferable. Or those having a cyclic molecular structure are preferred. As the silicone oil, those which are compatible with the crosslinkable silicone composition forming the crosslinked silicone particles are preferable. It is preferable that the silicone oil does not participate in the crosslinking reaction when forming the crosslinked silicone particles. When the crosslinked silicone particles are subjected to a hydrosilylation crosslinking reaction, an alkenyl group or a silicon atom bond is contained in the molecule. No hydrogen atom, for example, a dimethylpolysiloxane having a trimethylsiloxy group at both ends of a molecular chain, a methylphenylpolysiloxane having a trimethylsiloxy group at both ends of a molecular chain, a dimethylsiloxane having a trimethylsiloxy group at both ends of a molecular chain.
Methyl phenyl siloxane copolymer, dimethyl siloxane / methyl with trimethylsiloxy group capped at both molecular chains
(3,3,3-trifluoropropyl) siloxane copolymers, cyclic dimethylsiloxanes, and cyclic methylphenylsiloxanes. When the crosslinked silicone particles have been subjected to a condensation crosslinking reaction, silanol is contained in the molecule. In addition to the same silicone oils as described above, which have no groups, silicon-bonded hydrogen atoms or silicon-bonded hydrolyzable groups, for example, dimethylpolysiloxane having dimethylvinylsiloxy groups at both ends of the molecular chain, dimethylvinyl at both ends of the molecular chain Examples include a siloxy group-blocked dimethylsiloxane / methylvinylsiloxane copolymer, a trimethylsiloxy group-blocked methylvinylpolysiloxane at both molecular chain terminals, and a cyclic methylvinylsiloxane. The viscosity of such a silicone oil is 1 to 100,000,000 mPa ·
s, and more preferably 2 to 10,000,000 mPa · s at 25 ° C.

In this emulsion, the type of the organic oil is not limited, but those which are compatible with the crosslinkable silicone composition forming the crosslinked silicone particles are preferred. The organic oil is preferably an aliphatic oil having a molecular structure such as a linear, partially branched linear, cyclic, or branched chain, or an aromatic oil. Or an organic oil having a cyclic molecular structure. Further, this organic oil may have volatility. Such organic oils are preferably those that do not participate in the crosslinking reaction when forming the crosslinked silicone particles, and those having no alkenyl group in the molecule when the crosslinked silicone particles are those subjected to hydrosilylation crosslinking reaction. And, for example, alkanes such as hexane, heptane, paraffin, and isoparaffin; aromatics such as toluene and xylene; carbon tetrachloride;
Chlorinated compounds such as methylene chloride; ketones such as methyl isobutyl ketone; alcohols such as undecyl alcohol;
Examples thereof include ethers such as dibutyl ether; esters such as isopropyl laurate and isopropyl palmitate, and particularly preferably volatile alkanes. The viscosity of such an organic oil is preferably in the range of 1 to 100,000,000 mPa · s at 25 ° C, and in particular, 2 to 10,000, 25 ° C.
It is preferably within the range of 000 mPa · s.

[0012] Such a silicone oil or an organic oil may be used in combination with each other, or other components may be dissolved. By removing water and volatile silicone or organic oils from the emulsion of silicone or organic oils used, a mixture of cross-linked silicone particles with other components dissolved in the silicone or organic oils, or other Crosslinked silicone particles containing the components can be prepared. The other components that can be dissolved in the silicone oil or the organic oil are not particularly limited as long as they are soluble in the silicone oil or the organic oil. Organosilicon compounds such as rubber-like silicone oils; waxes such as carnauba wax, candelilla wax, mokuro, whale wax, jojoba oil, montan wax, beeswax, and lanolin; liquid paraffin, isoparaffin,
Hexyl laurate, isopropyl myristate, myristyl myristate, cetyl myristate, 2-octyldodecyl myristate, isopropyl palmitate,
2-ethylhexyl palmitate, butyl stearate, decyl oleate, 2-octyldodecyl oleate, myristyl lactate, cetyl lactate, lanolin acetate, stearyl alcohol, cetostearyl alcohol, oleyl alcohol, avocado oil, almond oil, olive oil,
Cacao oil, jojoba oil, sesame oil, safflower oil, soybean oil,
Oils such as camellia oil, squalane, persic oil, castor oil, mink oil, cottonseed oil, coconut oil, egg yolk oil, lard, etc .; glycol ester oils such as polypropylene glycol monooleate, neopentyl glycol-2-ethylhexanoate; isostearin Polyhydric alcohol ester oils such as acid triglyceride and coconut oil fatty acid triglyceride; and polyoxyalkylene ether oils such as polyoxyethylene lauryl ether and polyoxypropylene cetyl ether.

In this emulsion, the average particle size of the silicone oil or organic oil droplets is 0.1 to 50.
It is necessary to be within the range of 0 μm, preferably,
0.2 to 500 μm, more preferably,
In the range of 0.5 to 500 μm, particularly preferably
It is in the range of 0.5 to 200 μm. This tends to make it difficult to prepare an emulsion in which the average particle size of the droplets is less than the lower limit of the above range, whereas an emulsion exceeding the upper limit of the above range has reduced stability as a raw material for cosmetics. This is because there is a tendency.

In this emulsion, the average particle size of the crosslinked silicone particles must be in the range of 0.05 to 100 μm, and preferably in the range of 0.1 to 10 μm.
0 μm, particularly preferably 0.1 to 50.
It is in the range of μm. When the average particle size of the silicone oil or organic oil droplets is in the range of 0.2 to 500 μm, the average particle size of the crosslinked silicone particles is preferably in the range of 0.1 to 100 μm. It is particularly preferable that the thickness be in the range of 0.1 to 50 μm.
When the average particle size of the silicone oil or organic oil droplets is in the range of 0.5 to 500 μm, the average particle size of the crosslinked silicone particles is preferably in the range of 0.1 to 100 μm. It is particularly preferable that the thickness be in the range of 0.1 to 50 μm. Further, the average particle size of the silicone oil or organic oil droplets is 0.5 to 200.
When it is in the range of μm, the average particle size of the crosslinked silicone particles is preferably in the range of 0.1 to 100 μm, and particularly preferably in the range of 0.1 to 50 μm. This tends to make it difficult to prepare crosslinked silicone particles having an average particle size less than the lower limit of the above range, while crosslinked silicone particles exceeding the upper limit of the above range are not suitable for the stability of the emulsion as a cosmetic raw material. In addition, when blended with other cosmetic ingredients as a cosmetic ingredient, it is difficult to mix them uniformly, or the feel of the obtained cosmetic is insufficient.

The properties of the emulsion are liquid,
Cream and paste are exemplified. In this emulsion, the particle size of the crosslinked silicone particles is of course smaller than the particle size of the droplets of silicone oil or organic oil. The shape of the crosslinked silicone particles includes, for example, a sphere, a spindle shape, a flat shape, and an irregular shape, and is preferably a sphere.

As a method of preparing such an emulsion, for example, a crosslinkable silicone composition containing a non-crosslinkable silicone oil or an organic oil (however, the content of the non-crosslinkable silicone oil or the organic oil is Is more than the amount that the crosslinked product of the crosslinkable silicone composition can hold the non-crosslinkable silicone oil or organic oil.) Is dispersed in water to carry out a crosslinking reaction. The crosslinkable silicone composition that can be used in this method is preferably a composition that forms an elastomeric crosslinked product such as a rubber or gel by a crosslinking reaction. For example, a hydrosilylation crosslinking reaction type , Condensation cross-linking reaction type, organic peroxide cross-linking reaction type, high-energy ray cross-linking reaction type, preferably, hydrosilylation cross-linking reaction type, or condensation cross-linking reaction type It is.

Examples of the hydrosilylation crosslinking reaction type silicone composition include an organopolysiloxane having at least two alkenyl groups in one molecule and an organopolysiloxane having at least two silicon-bonded hydrogen atoms in one molecule. Examples include those comprising at least a siloxane and a catalyst for a hydrosilylation reaction. In this method, the crosslinkable silicone composition pre-mixed with the hydrosilylation reaction catalyst may be dispersed in water,
Further, after dispersing the crosslinkable silicone composition excluding this catalyst in water, the catalyst is added to water to prepare a crosslinkable silicone composition containing a hydrosilylation reaction catalyst in water. it can. At this time, it is preferable to use an aqueous dispersion in which the hydrosilylation reaction catalyst is dispersed to an average particle size of 1 μm or less.

The condensation-crosslinking reaction type silicone composition includes, for example, a hydroxyl group or an alkoxy group, an oxime group, and the like bonded to at least two silicon atoms in one molecule.
Organopolysiloxane having hydrolyzable groups such as acetoxy group and aminoxy group, silane having hydrolyzable groups such as alkoxy group, oxime group, acetoxy group and aminoxy group bonded to at least three silicon atoms in one molecule Examples include those comprising at least a system crosslinking agent and a condensation reaction catalyst such as an organotin compound and an organotitanium compound.

A filler may be added to the above-mentioned crosslinkable silicone composition as an optional component for adjusting the fluidity of the composition or improving the mechanical strength of the obtained crosslinked silicone particles. Examples of the filler include reinforcing fillers such as precipitated silica, fumed silica, calcined silica, and fumed titanium oxide; non-reinforcing fillers such as ground quartz, diatomaceous earth, aluminosilicate, iron oxide, zinc oxide, and calcium carbonate; A filler obtained by treating these surfaces with an organosilicon compound such as hexamethylsilazane, trimethylchlorosilane, polydimethylsiloxane, or polymethylhydrogensiloxane is exemplified.

The non-crosslinkable silicone oil contained in the crosslinkable silicone composition does not participate in the crosslinking reaction of the composition and is linear, partially branched linear, cyclic, or branched. Those having a molecular structure such as a chain are preferable, and those having a linear or cyclic molecular structure are particularly preferable. As this silicone oil,
Those which are compatible with the crosslinkable silicone composition are preferred. This non-crosslinkable silicone oil has no alkenyl group or silicon-bonded hydrogen atom in the molecule when the composition is a hydrosilylation crosslinkable reaction type, for example, a trimethylsiloxy group at both ends of the molecular chain. Dimethylpolysiloxane, molecular chain terminal trimethylsiloxy group-blocked methylphenylpolysiloxane, molecular chain terminal trimethylsiloxy group-blocked dimethylsiloxane / methylphenylsiloxane copolymer, molecular chain terminal trimethylsiloxy group-blocked dimethylsiloxane methyl (3, 3,
3-trifluoropropyl) siloxane copolymer, cyclic dimethylsiloxane, cyclic methylphenylsiloxane,
Glycidoxypropyl-modified polyorganosiloxane, and when the composition is a condensation-crosslinking reaction type, a silanol group, a silicon-bonded hydrogen atom, or a silicon-bonded hydrolyzable group in the molecule. In addition to the same silicone oils as described above, other than the above-mentioned silicone oils, for example, dimethylpolysiloxane having dimethylvinylsiloxy groups at both ends of molecular chains, dimethylsiloxane / methylvinylsiloxane copolymer having dimethylvinylsiloxy groups at both ends of molecular chains, It is a methylvinylpolysiloxane capped with a terminal trimethylsiloxy group, and a cyclic methylvinylsiloxane. Further, examples thereof include polyether-modified polyorganosiloxane modified with ethylene oxide and propylene oxide, and alkyl-modified polyorganosiloxane containing hexyl and dodecyl. The viscosity of such a non-crosslinkable silicone oil ranges from 1 to 100,000,000 at 25 ° C.
It is preferably within the range of 00 mPa · s,
It is preferably within the range of 2 to 10,000,000 mPa · s at 5 ° C.

The non-crosslinkable organic oil contained in the crosslinkable silicone composition does not participate in the crosslinking reaction of the composition, and is obtained by subjecting the crosslinked silicone particles to a hydrosilylation crosslinking reaction. In such a case, the compound does not have an alkenyl group in the molecule. The organic oil is preferably compatible with the crosslinkable silicone composition. Examples of such non-crosslinkable organic oils include alkanes such as hexane, heptane, paraffin, and isoparaffin; aromatics such as toluene and xylene; chlorinated compounds such as carbon tetrachloride and methylene chloride;
Ketones such as methyl isobutyl ketone; alcohols such as undecyl alcohol; ethers such as dibutyl ether; esters such as isopropyl laurate and isopropyl palmitate; and especially volatile alkane. preferable. The viscosity of such a non-crosslinkable organic oil is 1 to 100,00 at 25 ° C.
It is preferably in the range of 0.000 mPa · s, and particularly preferably in the range of 2 to 10,000,000 mPa · s at 25 ° C.

The content of the non-crosslinkable silicone oil or organic oil in the above-mentioned crosslinkable silicone composition is such that the crosslinked product of this crosslinkable silicone composition contains the non-crosslinkable silicone oil or organic oil in the crosslinked product. It is necessary that the amount exceeds the amount that can hold the oil, that is, the amount of the non-crosslinkable silicone oil or organic oil that can be contained in the crosslinked product. The amount that can be held is
Although it depends on the combination of the crosslinkable silicone composition and the non-crosslinkable silicone oil or organic oil, generally, based on 100 parts by weight of the crosslinkable silicone composition,
200 non-crosslinkable silicone or organic oils
It is preferably in the range of 5,000 to 5,000 parts by weight, and particularly preferably in the range of 250 to 2,000 parts by weight.

Further, in the non-crosslinkable silicone oil or organic oil in the crosslinkable silicone composition, other components may be dissolved in advance. As this component, those exemplified above can be mentioned. The content of other components that can be incorporated in the crosslinkable silicone composition varies depending on the combination of the crosslinkable silicone composition and the non-crosslinkable silicone oil or organic oil. Parts to other parts
Although it can be blended in the range of 001 to 200 parts by weight, it is preferably in the range of 0.1 to 50 parts by weight.

In this method, a crosslinkable silicone composition containing such a non-crosslinkable silicone oil or an organic oil is dispersed in water and then subjected to a crosslinking reaction. As a method of dispersing this crosslinkable silicone composition in water, there are a homomixer, a paddle mixer, a Henschel mixer, a homodisper, a colloid mill, a propeller stirrer, a homogenizer, an in-line continuous emulsifier, an ultrasonic emulsifier, and vacuum kneading. A method of dispersing the composition in water by an apparatus such as a machine is exemplified.

In this method, the amount of water used is not limited, but is preferably in the range of 5 to 99% by weight of the whole emulsion, particularly 10 to 80% by weight.
Is preferably within the range.

Further, in order to stably disperse the crosslinkable silicone composition in water, it is preferable to use a nonionic surfactant, a cationic surfactant, or an anionic surfactant. It is preferable to use system surface activity. Examples of the surfactant include silicone-based and organic-based surfactants.
It is preferably in the range of 0.1 to 20 parts by weight, especially 0.5 to 10 parts by weight, based on 100 parts by weight of the crosslinkable silicone composition containing a non-crosslinkable silicone oil or an organic oil. It is preferably within the range of parts.

By heating the emulsion of the crosslinkable silicone composition thus prepared, leaving it at room temperature, or irradiating it with a high energy ray,
The crosslinkable silicone composition dispersed in water can be crosslinked.

Further, the cosmetic raw material of the present invention may contain, as necessary, for example, liquid paraffin, isoparaffin, hexyl laurate, isopropyl myristate, myristyl myristate, cetyl myristate, myristate 2
-Octyldodecyl, isopropyl palmitate, 2-ethylhexyl palmitate, butyl stearate, decyl oleate, 2-octyldodecyl oleate, myristyl lactate, cetyl lactate, lanolin acetate, stearyl alcohol, cetostearyl alcohol, oleyl alcohol, avocado oil , Almond oil, olive oil, cocoa oil, jojoba oil, sesame oil, safflower oil, soybean oil, camellia oil, squalane, persic oil, castor oil, mink oil,
Glycol ester oils such as cottonseed oil, coconut oil, egg yolk oil, lard, polypropylene glycol monooleate, neopentyl glycol-2-ethylhexanoate; polyhydric alcohol ester oils such as isostearic acid triglyceride and coconut oil fatty acid triglyceride; Organic oils such as polyoxyalkylene ether oils such as ethylene lauryl ether and polyoxypropylene cetyl ether, and silicone oils may be separately blended.

The emulsion of the silicone oil or the organic oil can be prepared by dispersing the crosslinked silicone particles in the silicone oil or the organic oil and then emulsifying the dispersion. It is difficult to prepare an emulsion of silicone oil or organic oil in which the droplets are dispersed alone, and the silicone oil or organic oil dispersed in water contains crosslinked silicone particles in the droplets of the silicone oil or organic oil. Even if such a silicone oil or organic oil emulsion is used as a cosmetic raw material, the silicone oil or organic oil and the crosslinked silicone particles cannot be uniformly dispersed in cosmetics, and the silicone oil or organic oil must be uniformly dispersed. That is It was always difficult.

In the emulsion of silicone oil or organic oil prepared in this manner, the average particle size of the droplets of silicone oil or organic oil dispersed in water may be in the range of 0.1 to 500 μm. It is necessary, preferably in the range of 0.2 to 500 μm, more preferably in the range of 0.5 to 500 μm, and particularly preferably in the range of 0.5 to 200 μm. This tends to make it difficult to prepare an emulsion in which the average particle size of the droplets is less than the lower limit of the above range, whereas an emulsion exceeding the upper limit of the above range has reduced stability as a raw material for cosmetics. This is because there is a tendency.

In this emulsion, the average particle size of the crosslinked silicone particles must be in the range of 0.05 to 100 μm, preferably 0.1 to 10 μm.
0 μm, particularly preferably 0.1 to 50.
It is in the range of μm. When the average particle size of the silicone oil or organic oil droplets is in the range of 0.2 to 500 μm, the average particle size of the crosslinked silicone particles is preferably in the range of 0.1 to 100 μm. It is particularly preferable that the thickness be in the range of 0.1 to 50 μm.
When the average particle size of the silicone oil or organic oil droplets is in the range of 0.5 to 500 μm, the average particle size of the crosslinked silicone particles is preferably in the range of 0.1 to 100 μm. It is particularly preferable that the thickness be in the range of 0.1 to 50 μm. Further, the average particle size of the silicone oil or organic oil droplets is 0.5 to 200.
When it is in the range of μm, the average particle size of the crosslinked silicone particles is preferably in the range of 0.1 to 100 μm, and particularly preferably in the range of 0.1 to 50 μm. This is because there is a tendency that it is difficult to prepare crosslinked silicone particles having an average particle size less than the lower limit of the above range, while crosslinked silicone particles exceeding the upper limit of the above range are used as emulsions as cosmetic raw materials. This is because there is a tendency to decrease the stability of Of course, in this emulsion, the particle size of the crosslinked silicone particles is smaller than the particle size of the droplets of silicone oil or organic oil. The shape of the crosslinked silicone particles, for example, spherical, spindle shape, flat shape, irregular shape, and the like,
Preferably, it is spherical.

Further, an oil composition obtained by removing water from the emulsion thus prepared and having crosslinked silicone particles dispersed in silicone oil or organic oil can be used as a cosmetic raw material. Examples of a method for removing water from this emulsion include means such as air drying, hot air drying, vacuum drying, and heat drying. Such cosmetic raw materials are characterized in that crosslinked silicone particles are uniformly dispersed in silicone oil or organic oil, and the shape thereof is, for example, liquid, cream, paste, grease, powder, Alternatively, a lump-like form may be used. Cosmetic raw materials comprising such silicone oil compositions or organic oil compositions are useful as non-aqueous cosmetic raw materials.

Further, such cosmetic raw materials include, as necessary, for example, liquid paraffin, isoparaffin, hexyl laurate, isopropyl myristate, myristyl myristate, cetyl myristate, 2-octyldodecyl myristate, palmitic acid Isopropyl, 2-ethylhexyl palmitate, butyl stearate,
Decyl oleate, 2-octyldodecyl oleate,
Myristyl lactate, cetyl lactate, lanolin acetate, stearyl alcohol, cetostearyl alcohol, oleyl alcohol, avocado oil, almond oil, olive oil, cocoa oil, jojoba oil, sesame oil, safflower oil, soybean oil, camellia oil, squalane, persic oil , Castor oil, mink oil, cottonseed oil, coconut oil, egg yolk oil, lard, polypropylene glycol monooleate, neopentyl glycol-2-
Glycol ester oils such as ethylhexanoate; polyhydric alcohol ester oils such as isostearic acid triglyceride and coconut oil fatty acid triglyceride; organic oils such as polyoxyalkylene ether oils such as polyoxyethylene lauryl ether and polyoxypropylene cetyl ether; May contain silicone oil.

Next, the cosmetic of the present invention will be described in detail.
The cosmetic of the present invention is characterized by comprising a cosmetic raw material comprising the above-mentioned emulsion of silicone oil or organic oil and another cosmetic raw material. Examples of the cosmetics of the present invention include soaps, body shampoos, face-washing creams and other cleaning cosmetics, lotions, creams / milky lotions, basic cosmetics such as packs; Eyebrow cosmetics such as eye shadow, eye liner, mascara, makeup cosmetics such as nail polish; shampoo, hair rinse, hair conditioner, hair treatment, set lotion,
Hair cosmetics such as blow styling lotion, hair spray, foam styling agent, gel styling agent, hair liquid, hair tonic, hair cream, hair restorer, hair restorer, hair dye, hair styling agent, etc .; perfume, eau de cologne, etc. Aromatic cosmetics; toothpastes; bath agents; special cosmetics such as depilatory agents, shaving lotions, antiperspirants / deodorants, sunscreens, etc., and in particular, skin cosmetics such as basic cosmetics and make-up cosmetics; Hair cosmetics are preferred. In addition, as the dosage form of this cosmetic, aqueous liquid, oily liquid, emulsion, cream, foam, semi-solid,
Solid and powder forms are exemplified. This cosmetic can be used by spraying.

This cosmetic comprises a cosmetic raw material comprising an emulsion of silicone oil or organic oil containing the above-mentioned crosslinked silicone particles and another cosmetic raw material. Examples of the cosmetic raw material include avocado oil, almond oil, olive oil, Cocoa butter, sesame oil, wheat germ oil, safflower oil, shea butter, turtle oil, camellia oil, persic oil, castor oil, grape oil, macadamia nut oil, mink oil, egg yolk oil, mokuro, coconut oil, rosehip oil, hardened oil Waxes such as orange roughy oil, carnauba wax, candelilla wax, spermaceti, jojoba oil, montan wax, beeswax, lanolin; hydrocarbons such as liquid paraffin, vaseline, paraffin, ceresin, microcrystalline wax, squalane; laurin Acid, myristic acid, palmitic acid, Stearic acid, oleic acid, behenic acid, undecylenic acid, oxystearic acid, linoleic acid, lanolin acid, higher fatty acids such as synthetic fatty acids; ethyl alcohol, isopropyl alcohol, lauryl alcohol, cetyl alcohol, cetostearyl alcohol,
Stearyl alcohol, oleyl alcohol, behenyl alcohol, lanolin alcohol, hydrogenated lanolin alcohol, hexyldecanol, octyldodecanol, isostearyl alcohol, etc .; cholesterol, dihydrocholesterol, phytosterol, etc. sterol; ethyl linoleate, isopropyl myristate, isopropyl lanolin fatty acid , Hexyl laurate, myristyl myristate, cetyl myristate, octyl dodecyl myristate, decyl oleate, octyl dodecyl oleate, hexyl decyl dimethyl octanoate, cetyl isooctanoate, cetyl palmitate, glyceryl trimyristate, tri (capryl. Capric acid) glycerin, propylene glycol dioleate, triisoste Glycerophosphate, triisooctanoate glycerin, cetyl lactate, myristyl lactate,
Fatty acid esters such as diisostearyl malate; glycerin, propylene glycol, 1,3-butylene glycol, polyethylene glycol, sodium d, l-pyrrolidonecarboxylate, sodium lactate, sorbitol,
Moisturizers such as sodium hyaluronate; higher fatty acid soaps,
Anionic surfactants such as higher alcohol sulfates, N-acyl glutamates and phosphates, cationic surfactants, amphoteric surfactants such as betaines, amino acids, imidazolines and lecithin, polyhydric alcohol esters Surfactants such as non-ionic surfactants such as ethylene oxide condensation type; colored pigments such as iron oxide; white pigments such as zinc oxide, titanium oxide and zirconium oxide; extender pigments such as mica, talc and sericite. Pigment; silicone oil such as dimethylpolysiloxane, methylphenylpolysiloxane, octamethyltetracyclosiloxane, decamethylcyclopentasiloxane, polyether-modified silicone oil, amino-modified silicone oil; purified water;
Thickeners such as carrageenan, alginic acid, gum arabic, tragacanth, pectin, starch, xanthan gum, polyvinyl alcohol, polyvinylpyrrolidone, sodium polyacrylate, polyethylene glycol, and the like,
Examples include UV absorbers, antibacterial agents, anti-inflammatory agents, antiperspirants, preservatives, fragrances, antioxidants, pH adjusters, and propellants.

When the cosmetic is a hair cosmetic, the other hair cosmetic raw materials include fats and oils, surfactants,
Examples of the fats and oils that can contain a film forming agent, an antidandruff agent, an antioxidant, a wetting agent, and the like include waxes such as microcrystalline wax, paraffin wax, gay wax, beeswax, Japan wax, and sucrose wax. Or mixtures thereof; liquid paraffin, α-
Olefin oligomers, squalane, hydrocarbon oils such as squalene, or mixtures thereof; linear or branched, saturated or unsaturated, such as cetanol, stearyl alcohol, isostearyl alcohol, hydrogenated castor oil derived alcohol, behenyl alcohol, lanolin alcohol, Hydroxy-substituted or unsubstituted higher alcohols,
Or mixtures thereof; palmitic acid, myristic acid,
Oleic acid, stearic acid, hydroxystearic acid,
Linear or branched, saturated or unsaturated, hydroxy-substituted or unsubstituted higher fatty acids such as isostearic acid, behenic acid, castor oil fatty acid and coconut oil fatty acid, or mixtures thereof; olive oil, coconut oil, rapeseed oil, palm oil , Palm kernel oil, castor oil, hardened castor oil, peanut oil, beef tallow, hydrogenated tallow, jojoba oil, hardened jojoba oil, monostearic acid glyceride, monooleic acid glyceride, dipalmitic acid glyceride, trimmyristic acid glyceride, oleyl oleate Esters such as isostearyl isostearate, palmityl behenate, isopropyl palmitate, stearyl acetate, dihydroxystearate; linear, branched, or cyclic low molecular weight silicone oil; amino-modified silicone oil; Fatty acid modified sily N'oiru, alcohol-modified silicone oil, polyether-modified silicone oil,
Silicone oils such as phosphoric acid (salt) group-containing silicone oil, sulfate (salt) group-containing silicone oil, fluorine-modified alkyl group-containing silicone oil, alkyl-modified silicone oil, and epoxy-modified silicone oil; soluble in solvents and liquid at room temperature And a raw rubber-like high molecular weight silicone oil, a thermoplastic silicone resin, or a mixture thereof.

Examples of the surfactant include glycerin fatty acid esters such as glycerin monostearate; sorbitan fatty acid esters such as sorbitan monopalmitate; polyoxyethylene alkyl ethers such as polyoxyethylene cetyl ether; polyoxyethylene stearic acid Polyoxyethylene fatty acid esters such as esters and polyoxyethylene sorbitan monolaurate; and other nonionic surfactants such as polyoxyethylene alkyl phenyl ether, polyoxyethylene castor oil, polyoxyethylene hydrogenated castor oil, and fatty acid alkylolamide Agents; monoalkyltrimethylammonium salts such as stearyltrimethylammonium chloride and behenyltrimethylammonium chloride; distearyldimethylammonium chloride; Cationic surfactants such as dialkyl dimethyl ammonium salts such as f alkenyl dimethyl ammonium, or amphoteric surfactants.

Examples of the film forming agent include a polymer of a (meth) acrylic radical polymerizable monomer, a copolymer with a silicone compound, poly (N-acylalkylenimine), and poly (N-methylpyrrolidone). And a silicone resin modified with a fluorine group-containing organic group or an amino group, and an unmodified silicone resin. Examples of the anti-dandruff agent include sulfur, selenium sulfide, zinc pyrithione, octopirox, zinc pyridium-1-thiol-N
-Oxide, salicylic acid, 2,4,4'-trichloro-2'-hydroxydiphenyl ether, 1-hydroxy-2-pyridone compounds. Examples of the antioxidant include BHA, BHT, and γ-oryzanol. Examples of the wetting agent include hexylene glycol, polyethylene glycol, sodium pyroglutamate, propylene glycol, sorbitol, and glycerin.

Further, in hair cosmetics, as other optional components, feel-improving agents such as squalene, lanolin, perfluoropolyether, and cationic polymer; ethanol, isopropyl alcohol, 1,3-butylene glycol, ethylene glycol, propylene Antifreezing agents such as glycol and glycerin; chelating agents such as ethylenediaminetetraacetic acid, citric acid, ethane-1-hydroxy-1,1-diphosphonic acid, and salts thereof;
Benzophenone derivatives such as hydroxy-4-methoxybenzophenone, 2- (2′-hydroxy-5′-methyl-
Benzotriazole derivatives such as phenyl) -benzotriazole, ultraviolet absorbers such as cinnamate; fungicides such as triclosan and trichlorocarban; anti-inflammatory agents such as potassium glycyrrhizinate and tocopherol acetate; preservatives such as methylparaben and butylparaben; Coloring agents such as pearling agents, pigments, dyes, etc .; sprays, vitamins, hair tonics, hormones, fragrances, etc.
Shampoo Ingredients (Micel
le press, 1985).

When the hair cosmetic is water-based, xanthan gum, guar gum, carboxymethylcellulose, polyvinyl alcohol, polyvinylpyrrolidone, carboxyvinyl polymer are used in addition to water such as purified water for dispersion stabilization or hair styling. And water-soluble polymers such as hydroxyethylcellulose and polyoxyethylene glycol distearate, and these water-soluble polymers or ethanol as a viscosity modifier for aqueous hair cosmetics.

In the cosmetic of the present invention, the amount of the cosmetic raw material composed of the emulsion of silicone oil or organic oil as described above is 0.1 to 99% in terms of components other than water (in terms of solid content). It is preferably 0.9% by weight, and particularly preferably in the range of 0.5 to 99% by weight. This is because if the amount of the cosmetic raw material composed of the emulsion exceeds the upper limit of the above range, the effect as a cosmetic tends to be lost, while if the amount is less than the lower limit of the above range, This is because blending of the emulsion tends to make it difficult to improve the feeling of use of cosmetics.

The cosmetic of the present invention is characterized by comprising a cosmetic raw material comprising the above oil composition and another cosmetic raw material. The cosmetic raw materials comprising the oil composition are as described above. Also, as other cosmetic ingredients,
The same raw materials as described above are exemplified.

In this cosmetic, the compounding amount of the cosmetic comprising the above oil composition is 0.5 to 9% in the cosmetic.
It is preferably in the range of 9.0% by weight, especially 1.0% by weight.
Preferably it is in the range of 0 to 95% by weight. This is because if the amount of the cosmetic raw material composed of the oil composition exceeds the upper limit of the above range, the effect as a cosmetic tends to be lost. This is because the use feeling and the like of cosmetics tend to be hardly improved by blending the above oil composition.

Next, the method for producing the cosmetic of the present invention will be described in detail. The production method of the present invention is characterized in that a cosmetic material comprising the above-mentioned emulsion of silicone oil or organic oil is blended with another cosmetic material. ADVANTAGE OF THE INVENTION According to the manufacturing method of the cosmetics of this invention, a silicone oil or an organic oil and a crosslinked silicone powder can be uniformly disperse | distributed in cosmetics without applying a special apparatus or high shear. In the production method of the present invention, for example, cosmetics are produced by a batch method or a continuous method. Examples of apparatuses used in such a method include a homomixer, a paddle mixer, a Henschel mixer, a homodisper, a colloid mill, a propeller stirrer, and a homogenizer. , An in-line continuous emulsifier, an ultrasonic emulsifier, and a vacuum kneader.

In the cosmetic of the present invention, after mixing the above-mentioned cosmetic raw material comprising an emulsion of silicone oil or organic oil and part or all of other cosmetic raw materials, water is removed, and Further, by blending other cosmetic raw materials, it is possible to prepare a cosmetic in which silicone oil or organic oil and crosslinked silicone particles are uniformly dispersed. In this method, examples of the method of removing water include a method of depressurizing, heating, or air drying, and a method of contacting with a water absorbent.

This cosmetic comprises a cosmetic raw material comprising an emulsion of silicone oil or organic oil containing the above-mentioned cross-linked silicone particles and other cosmetic raw materials, which include avocado oil, almond oil, olive oil, Cocoa butter, sesame oil, wheat germ oil, safflower oil, shea butter, turtle oil, camellia oil, persic oil, castor oil, grape oil, macadamia nut oil, mink oil, egg yolk oil, mokuro, coconut oil, rosehip oil, hardened oil Waxes such as orange roughy oil, carnauba wax, candelilla wax, spermaceti, jojoba oil, montan wax, beeswax, lanolin; hydrocarbons such as liquid paraffin, vaseline, paraffin, ceresin, microcrystalline wax, squalane; laurin Acid, myristic acid, palmitic acid, Stearic acid, oleic acid, behenic acid, undecylenic acid, oxystearic acid, linoleic acid, lanolin acid, higher fatty acids such as synthetic fatty acids; ethyl alcohol, isopropyl alcohol, lauryl alcohol, cetyl alcohol, cetostearyl alcohol,
Stearyl alcohol, oleyl alcohol, behenyl alcohol, lanolin alcohol, hydrogenated lanolin alcohol, hexyldecanol, octyldodecanol, isostearyl alcohol, etc .; cholesterol, dihydrocholesterol, phytosterol, etc. sterol; ethyl linoleate, isopropyl myristate, isopropyl lanolin fatty acid , Hexyl laurate, myristyl myristate, cetyl myristate, octyl dodecyl myristate, decyl oleate, octyl dodecyl oleate, hexyl decyl dimethyl octanoate, cetyl isooctanoate, cetyl palmitate, glyceryl trimyristate, tri (capryl. Capric acid) glycerin, propylene glycol dioleate, triisoste Glycerophosphate, triisooctanoate glycerin, cetyl lactate, myristyl lactate,
Fatty acid esters such as diisostearyl malate; glycerin, propylene glycol, 1,3-butylene glycol, polyethylene glycol, sodium d, l-pyrrolidonecarboxylate, sodium lactate, sorbitol,
Moisturizers such as sodium hyaluronate; higher fatty acid soaps,
Anionic surfactants such as higher alcohol sulfates, N-acyl glutamates and phosphates, cationic surfactants, amphoteric surfactants such as betaines, amino acids, imidazolines and lecithin, polyhydric alcohol esters Surfactants such as non-ionic surfactants such as ethylene oxide condensation type; colored pigments such as iron oxide; white pigments such as zinc oxide, titanium oxide and zirconium oxide; extender pigments such as mica, talc and sericite. Pigment; silicone oil such as dimethylpolysiloxane, methylphenylpolysiloxane, octamethyltetracyclosiloxane, decamethylcyclopentasiloxane, polyether-modified silicone oil, amino-modified silicone oil; purified water;
Thickeners such as carrageenan, alginic acid, gum arabic, tragacanth, pectin, starch, xanthan gum, polyvinyl alcohol, polyvinylpyrrolidone, sodium polyacrylate, polyethylene glycol, and the like,
Examples include UV absorbers, antibacterial agents, anti-inflammatory agents, antiperspirants, preservatives, fragrances, antioxidants, pH adjusters, and propellants.

In the cosmetics of the present invention, the amount of the cosmetic raw material composed of the emulsion of silicone oil or organic oil as described above is 0.1 to 99% in terms of components other than water (in terms of solid content). It is preferably 0.9% by weight, and particularly preferably in the range of 0.5 to 99% by weight. This is because when the amount of the cosmetic raw material composed of the silicone oil or organic oil emulsion exceeds the upper limit of the above range, the cosmetic effect tends to be lost.
If the amount is less than the lower limit of the above range, the feeling of use of cosmetics or the like by blending an emulsion of silicone oil or organic oil tends to be difficult to be improved.

[0048]

EXAMPLES Cosmetic raw materials, cosmetics, and a method for producing cosmetics according to the present invention will be described in detail with reference to Examples. In addition, the viscosity in an Example is a value in 25 degreeC.

The average particle size and stability of the silicone oil emulsion, the average particle size of the crosslinked silicone particles, and the characteristics of the silicone oil composition were determined as follows. [Average particle size of silicone oil emulsion] Laser diffraction particle size distribution analyzer
(LA-500 of Horiba, Ltd.), and the obtained median diameter (particle diameter corresponding to 50% of the cumulative distribution) was defined as the average particle diameter. [Stability of Silicone Oil Emulsion] 180 mL of the silicone oil emulsion was sealed in a 225 mL glass bottle (105 mm in depth, 50 mm in diameter) and allowed to stand at room temperature for 1 week. After standing, the thickness of the aqueous layer separated from the silicone oil emulsion was measured. [Dispersibility of Crosslinked Silicone Particles] The silicone oil emulsion was air-dried on a glass plate and observed under a stereoscopic microscope for the shape, aggregation state, and distribution of the crosslinked silicone particles. If all the crosslinked silicone particles are dispersed as primary particles, the result is evaluated as “○”, and several hundred μm aggregated particles or 500
If there were primary particles of μm or more, it was marked as x, and between these was marked as Δ. [Average Particle Size of Crosslinked Silicone Particles] A silicone oil emulsion was air-dried in a glass plate shape, and a crosslinked silicone particle was collected under a stereoscopic microscope to prepare a sample, which was observed under an electron microscope. The average particle size was determined from the above. [Viscoelasticity of Silicone Oil Composition] The storage elastic modulus G ′ (× 10 ³ dyne / cm ² ), loss elastic modulus G ″ (× 10 ³ dyne / cm ² ), and loss tangent tan δ of the silicone oil composition were determined. ARES
Viscoelasticity measuring device (Reometric Scienti
fic). The measurement conditions were room temperature, 25 mm parallel plate, gap: 0.5 to 0.6.
mm, strain: 10%, frequency: 0.1 to 50 rad / s.

[Preparation of Cosmetic Raw Materials] Cosmetic raw materials (A) to
(D) was prepared as follows. The properties of these cosmetic raw materials are shown in Table 1. [Reference Example 1] Dimethylvinylsiloxy-group-blocked dimethylpolysiloxane having a viscosity of 400 mPa · s at both ends of a molecular chain, 18.8
1.2 parts by weight of a dimethylsiloxane-methylhydrogensiloxane copolymer (content of silicon-bonded hydrogen atoms = 0.5% by weight) having a trimethylsiloxy group at both ends of the molecular chain having a viscosity of 30 mPa · s and a viscosity of 100 mPa A crosslinkable silicone composition was prepared by mixing 80 parts by weight of dimethylpolysiloxane capped with trimethylsiloxy groups at both ends of the molecular chain of s. Next, 3% by weight was added to the crosslinkable silicone composition.
-Polyoxyethylene nonyl phenyl ether (HLB
= 13.1) After adding 53 parts by weight of an aqueous solution and emulsifying with a colloid mill, 50 parts by weight of pure water was further added to prepare an aqueous emulsion of a crosslinkable silicone composition.

A separately prepared aqueous emulsion of a platinum-based catalyst containing 1,1-divinyl-1,1,3,3-tetramethoxydisiloxane complex of platinum as a main component (average particle diameter of platinum-based catalyst) = 0.05 μm, platinum metal concentration = 0.0
5% by weight) was added to the aqueous emulsion of the crosslinkable silicone composition described above in an amount such that the amount of platinum metal was 20 ppm by weight based on the dimethylpolysiloxane blocked with dimethylvinylsiloxy groups at both molecular chains in the emulsion. To form an aqueous emulsion of a crosslinkable silicone composition.

The emulsion is allowed to stand at room temperature for one day to perform a hydrosilylation crosslinking reaction of the crosslinkable silicone composition, and the silicone oil containing the crosslinked silicone particles in the silicone oil droplets dispersed in water. An emulsion was prepared and used as a cosmetic raw material (A).

Next, the emulsion was transferred to an aluminum dish having a diameter of 5 cm and air-dried in a fume hood for 3 days to remove water, thereby preparing a silicone oil composition comprising silicone oil and crosslinked silicone particles. This silicone oil composition was creamy. Observation of the silicone oil composition with a stereomicroscope revealed that the crosslinked silicone particles were uniformly dispersed in the silicone oil, and the shape of the crosslinked silicone particles was spherical.

Reference Example 2 In Reference Example 1, the viscosity was 10
Instead of 80 parts by weight of dimethylpolysiloxane capped with trimethylsiloxy groups at both ends of the molecular chain of 0 mPa · s, the viscosity was 6 mPa · s.
An aqueous emulsion of a crosslinkable silicone composition was prepared in the same manner as in Reference Example 1 except that 80 parts by weight of dimethylpolysiloxane capped with trimethylsiloxy groups at both ends of the molecular chain of s was used. This emulsion was subjected to a hydrosilylation crosslinking reaction in the same manner as in Reference Example 1 to prepare a silicone oil emulsion containing silicone oil droplets in silicone oil droplets dispersed in water.

Next, water was removed from this emulsion in the same manner as in Reference Example 1 to prepare a silicone oil composition comprising silicone oil and crosslinked silicone particles, which was used as a cosmetic raw material (B). This silicone oil composition was creamy. Observation of the silicone oil composition with a stereomicroscope revealed that the crosslinked silicone particles were uniformly dispersed in the silicone oil, and the shape of the crosslinked silicone particles was spherical.

REFERENCE EXAMPLE 3 100 parts by weight of a dimethylpolysiloxane having a hydroxyl group-terminated hydroxyl group having a viscosity of 1,000 mPa · s (having a hydroxyl group content of 1.3% by weight) and a trimethyl group-terminated molecular chain having a viscosity of 10 mPa · s 10 parts by weight of siloxy group-blocked methyl hydrogen polysiloxane (content of silicon-bonded hydrogen atoms = 1.5% by weight), 50 parts by weight of dimethylpolysiloxane blocked with trimethylsiloxy group at both ends of molecular chain having a viscosity of 1,000 mPa · s The mixture was uniformly mixed to prepare mixture (I).

A dimethylpolysiloxane having a viscosity of 1,000 mPa · s and a hydroxyl group at both ends of a molecular chain (hydroxyl content =
(1.3% by weight) 100 parts by weight, 50 parts by weight of dimethylpolysiloxane endblocked by trimethylsiloxy groups at both molecular chains having a viscosity of 1,000 mPa · s, and 1.5 parts by weight of dibutyltin dioctate
The parts by weight were uniformly mixed to prepare a mixture (II).

The mixture (I) and the mixture (II) were mixed at a weight ratio of 1:
After mixing uniformly with No. 1, add Tergitol TMN-6 to this.
(Ethylene oxide adduct of trimethylnonanol, manufactured by Union Carbide) 5% by weight and ion-exchanged water 1.7
00 parts by weight of the mixture was added and emulsified by a colloid mill. This emulsion is spray-dried (entrance temperature: 3
(00 ° C., outlet temperature: 100 ° C.) to remove water, whereby crosslinked silicone particles could be obtained in a yield of 98%. This was designated as cosmetic raw material (C). The crosslinked silicone particles were rubber-like, and the shape was spherical.
No bleeding of silicone oil from the crosslinked silicone particles was observed.

Reference Example 4 A planetary mixer was charged with 44.5 parts by weight of a dimethylpolysiloxane having a viscosity of 5 mPa · s and a vinylmethylsiloxy group at both ends of a molecular chain, and a viscosity of 20 mPa · s.
100 parts by weight of methyl hydrogen polysiloxane (both containing silicon-bonded hydrogen atoms = 1.5% by weight) having a molecular chain at both ends and having a viscosity of 6 mPa · s. After mixing 758 parts by weight, 2 parts of chloroplatinic acid was added thereto.
A cross-linkable silicone composition was prepared by adding 0.5 parts by weight of a% by weight-isopanol solution. By stirring this crosslinkable silicone composition for 2 hours while heating it to 70 to 80 ° C., a hydrosilylation crosslinking reaction of the crosslinkable silicone composition was performed to prepare a soft silicone composition. When this silicone composition was kneaded under shearing force with three rolls, a paste-like silicone composition was prepared. This was designated as cosmetic raw material (D). When the silicone composition was observed with a stereomicroscope, irregularly-shaped crosslinked silicone particles were dispersed in the silicone oil, but the dispersion was uneven, and the particle size of the crosslinked silicone particles was about 100 to 500 μm. It turned out to be big.

[0060]

[Table 1]

[Production Method of Cosmetics and Cosmetics] Cosmetics were prepared as follows, and their characteristics were evaluated. [Feeling of Cosmetics to Fingers] When 10 panelists used the cosmetics and the number of people who felt that the cosmetics felt good was 8 to 10 people, and when this was 4 to 7 people. Δ, and the case of three or less was evaluated as x. [Feeling of cosmetics on the skin] When 10 panelists used the cosmetics and the number of people who felt that the cosmetics had a good feeling was 8 to 10 people, and when this was 4 to 7 people Δ, and the case of three or less was evaluated as x. [Dispersion state of crosslinked particles in cosmetics] Cosmetic products are thinly applied on a glass plate, the particle size of the crosslinked silicone particles in the cosmetics is observed by an optical microscope, and the ratio of the crosslinked silicone particles having a particle size of 10 µm or less is determined. Over 10 μm,
Ratio of crosslinked silicone particles of 50 μm or less, 50 μm
The dispersibility of the crosslinked silicone particles in cosmetics was evaluated by determining the ratio of the crosslinked silicone particles exceeding m, respectively.

Example 1 52 parts by weight of cosmetic raw material (A)
5 parts by weight of octyl p-methoxycinnamate, 1 part by weight of α-monoisostearyl glyceryl ether polyoxyethylene sorbitan monooleate, 2 parts by weight of beeswax, 2 parts by weight of lanolin, 10 parts by weight of squalane, 10 parts by weight of liquid paraffin, 19 parts by weight of purified water, appropriate amount of preservative,
An appropriate amount of the perfume was stirred with a homodisper at 2500 rpm for 3 minutes to prepare an emulsion cosmetic. Table 2 shows the evaluation results of the cosmetic.

Example 2 52 parts by weight of cosmetic raw material (B)
5 parts by weight of octyl p-methoxycinnamate, 1 part by weight of α-monoisostearyl glyceryl ether polyoxyethylene sorbitan monooleate, 2 parts by weight of beeswax, 2 parts by weight of lanolin, 10 parts by weight of squalane, 10 parts by weight of liquid paraffin, 19 parts by weight of purified water, appropriate amount of preservative,
An appropriate amount of the perfume was stirred with a homodisper at 2500 rpm for 3 minutes to prepare an emulsion cosmetic. Table 2 shows the evaluation results of the cosmetic.

[Comparative Example 1] An emulsion of dimethylpolysiloxane having a viscosity of 100 mPa · s and capped with trimethylsiloxy groups at both ends of the molecular chain (concentration: 50 wt%) ) 12 parts by weight,
24 parts by weight, 5 parts by weight of octyl p-methoxycinnamate, α
Monoisostearyl glyceryl ether polyoxyethylene sorbitan monooleate 1 part by weight, beeswax 2 parts by weight, lanolin 2 parts by weight, squalane 10 parts by weight, liquid paraffin 10 parts by weight, purified water 54 parts by weight,
Appropriate amount of preservative and perfume are added by homodisper 2
The mixture was stirred at 500 rpm for 3 minutes to prepare an emulsion cosmetic.
Table 2 shows the evaluation results of the cosmetic.

[0065]

[Table 2]

Example 3 40 parts by weight of cosmetic raw material (B)
1 part by weight of silicon-treated titanium oxide, 5 parts by weight of octyl p-methoxycinnamate, 10 parts by weight of dimethylpolysiloxane having a viscosity of 20 mPa · s and capped with trimethylsiloxy groups at both molecular terminals, polyoxyethylene (40 mol adduct) hydrogenated castor oil 3 parts by weight, 30 parts by weight of squalane, 5 parts by weight of glycerin, 3 parts by weight of beeswax, an appropriate amount of preservative, an appropriate amount of perfume, and an appropriate amount of purified water were stirred with a Henschel mixer at 1500 rpm for 5 minutes to prepare a creamy cosmetic. Table 3 shows the evaluation results of this cosmetic.

Comparative Example 2 20 parts by weight of a cosmetic raw material (D)
1 part by weight of silicon-treated titanium oxide, 5 parts by weight of octyl p-methoxycinnamate, 10 parts by weight of dimethylpolysiloxane having a viscosity of 20 mPa · s and capped with trimethylsiloxy groups at both molecular terminals, polyoxyethylene (40 mol adduct) hydrogenated castor oil 3 parts by weight, 30 parts by weight of squalane, 5 parts by weight of glycerin, 3 parts by weight of beeswax, an appropriate amount of preservative, an appropriate amount of perfume, and an appropriate amount of purified water were stirred with a Henschel mixer at 1500 rpm for 5 minutes to prepare a creamy cosmetic. Table 3 shows the evaluation results of this cosmetic.

[0068]

[Table 3]

Example 4 14 parts by weight of a cosmetic raw material (B)
1,3-butylene glycol 2 parts by weight, ethanol 50
Parts by weight, polyether-modified silicone oil (SH3771 manufactured by Dow Corning Toray Silicone Co., Ltd.)
1 part by weight, propylene glycol 4 parts by weight, polyoxyethylene (15 mol adduct) nonyl ether 1 part by weight,
1 part by weight of siliconized titanium oxide, trace amount of preservative, trace amount of fragrance, and purified water
An aqueous cosmetic was prepared by stirring at 500 rpm for 5 minutes. Table 4 shows the evaluation results of the cosmetic.

Comparative Example 3 2 parts by weight of an emulsion (concentration: 50% by weight) of a dimethylpolysiloxane having a viscosity of 100 mPa · s and capped at both ends of a molecular chain with a methylmethylsiloxane concentration of 1 part by weight, and 4 parts by weight of purified water , 1,3-butylene glycol 2 parts by weight, ethanol 50 parts by weight, polyether-modified silicone oil (SH3771 manufactured by Dow Corning Silicone Toray Co., Ltd.) 1 part by weight, propylene glycol 4 parts by weight, polyoxyethylene (15 mol Additives) An aqueous cosmetic was prepared by stirring 1 part by weight of oil ether, 1 part by weight of siliconized titanium oxide, a trace amount of preservative, trace amount of perfume, and an appropriate amount of purified water at 1500 rpm for 5 minutes using a Henschel mixer. Table 4 shows the evaluation results of the cosmetic.

[0071]

[Table 4]

Example 5 The cosmetic raw material (A) prepared in Reference Example 1 was spread on a metal dish to a thickness of 5 mm and air-dried for one week at room temperature, so that the crosslinked silicone particles were uniformly dispersed in the silicone oil. A dispersed paste-like silicone oil composition was prepared. This silicone composition was used as a cosmetic raw material (A ′). 105 ° C of this cosmetic raw material (A '), 3
The loss on heating after heating for 0 minutes was 0.2% by weight.

A cosmetic raw material (A ′) (10 parts by weight), decamethylcyclopentasiloxane (10 parts by weight), silicone-treated titanium dioxide (10 parts by weight), and an appropriate amount of a fragrance were mixed with a Henschel mixer, and the mixture was mixed with silicone-treated zinc white (5 parts by weight). 55 parts by weight of silicone-treated talc, a silicone-treated pigment and an appropriate amount of perfume were mixed to prepare a rouge. The properties of this blusher are shown in Table 5.

Comparative Example 4 A blusher was prepared in the same manner as in Example 5, except that the cosmetic raw material (D) was used instead of the cosmetic raw material (A ′). The properties of this blusher are shown in Table 5.

[0075]

[Table 5]

Example 6 100 parts by weight of the cosmetic raw material (B) prepared in Reference Example 2 and 10 parts by weight of a silicone rubber powder having an average particle diameter of 4 μm (Trefle E-506C manufactured by Dow Corning Toray Silicone Co., Ltd.) After mixing the parts with a planetary mixer, the water was removed by reducing the pressure at 50 ° C.,
A uniform paste-like silicone oil composition was prepared.
This paste-like silicone oil composition has a viscosity of 3 ° C at 105 ° C.
The loss on heating after heating for 0 minutes was 0.3% by weight or less. 40 parts by weight of this paste-form silicone oil composition, 10 parts by weight of sericite, 10 parts by weight of siliconized titanium dioxide, 1.5 parts by weight of siliconized bengara,
Silicone-treated yellow iron oxide 4 parts by weight, siliconized black iron oxide 0.3 parts by weight, Aristo wax 4 parts by weight, carnauba wax 1.3 parts by weight, squalane 33 parts by weight, sorbitan sesquioleate 1 part by weight, kaolin 3 parts by weight ,
An appropriate amount of the fragrance was mixed with a Henschel mixer to prepare a foundation. Table 6 shows the characteristics of the foundation.

Comparative Example 5 A foundation was prepared in the same manner as in Example 6, except that the same amount of the cosmetic raw material (D) was used instead of the paste-like silicone oil composition. Table 6 shows the characteristics of the foundation.

[0078]

[Table 6] * The dispersion of the crosslinked silicone particles in Comparative Example 5 shows the silicone rubber powder blended as another cosmetic raw material.
(E-506C) is also included.

[Preparation of Hair Cosmetic Raw Materials] Hair Cosmetic Raw Materials
(E) to (J) were prepared as follows. The properties of these hair cosmetic raw materials are shown in Table 7. [Reference Example 5] Dimethylvinylsiloxy group-blocked dimethylpolysiloxane having a viscosity of 400 mPa · s at both ends of dimethylpolysiloxane 15.7
1.0 parts by weight of a dimethylsiloxane-methylhydrogensiloxane copolymer (content of silicon-bonded hydrogen atoms = 0.5% by weight) having a trimethylsiloxy group at both ends of the molecular chain having a viscosity of 30 mPa · s and a viscosity of 20 mPa A crosslinkable silicone composition was prepared by mixing 83.3 parts by weight of dimethylpolysiloxane having a trimethylsiloxy group at both ends of the molecular chain of s. Next, 3% by weight of polyoxyethylene nonylphenyl ether (HL) was added to the crosslinkable silicone composition.
B = 13.1) After adding 53 parts by weight of an aqueous solution and emulsifying by a colloid mill, 50 parts by weight of pure water was further added to prepare an aqueous emulsion of a crosslinkable silicone composition.

A separately prepared aqueous emulsion of a platinum-based catalyst containing 1,1-divinyl-1,1,3,3-tetramethoxydisiloxane complex of platinum as a main component (average particle diameter of platinum-based catalyst) = 0.05 μm, platinum metal concentration = 0.0
5% by weight) was added to the aqueous emulsion of the crosslinkable silicone composition described above in an amount such that the amount of platinum metal was 20 ppm by weight based on the dimethylpolysiloxane blocked with dimethylvinylsiloxy groups at both molecular chains in the emulsion. To form an aqueous emulsion of a crosslinkable silicone composition.

By leaving this emulsion at room temperature for one day, a hydrosilylation cross-linking reaction of the cross-linkable silicone composition is performed, and a silicone oil containing cross-linked silicone particles in silicone oil droplets dispersed in water. Prepare emulsion and use it as raw material for hair cosmetics
(E).

Next, the emulsion was transferred to an aluminum dish having a diameter of 5 cm and air-dried in a fume hood for 3 days to remove water, thereby preparing a silicone oil composition comprising silicone oil and crosslinked silicone particles. This silicone oil composition was creamy. Observation of the silicone oil composition with a stereomicroscope revealed that the crosslinked silicone particles were uniformly dispersed in the silicone oil, and the shape of the crosslinked silicone particles was spherical.

[Reference Example 6] In Reference Example 5, the viscosity was 20
80 parts by weight of decamethylpentasiloxane and a viscosity of 20,000,000 mPa · s instead of 83.3 parts by weight of dimethylpolysiloxane capped with trimethylsiloxy groups at both ends of the molecular chain of mPa · s
Cross-linkable silicone composition in the same manner as in Reference Example 5 except that 83.3 parts by weight of a mixture comprising 3.3 parts by weight of a dimethylpolysiloxane endblocked by trimethylsiloxy groups at both ends of the molecular chain and having a viscosity of 300 mP · s was used. Was prepared. This emulsion was subjected to a hydrosilylation crosslinking reaction in the same manner as in Reference Example 5 to prepare a silicone oil emulsion containing silicone oil droplets dispersed in water in silicone oil droplets.

Next, water was removed from this emulsion in the same manner as in Reference Example 5 to prepare a silicone oil composition comprising silicone oil and crosslinked silicone particles, which was used as a hair cosmetic raw material (F). This silicone oil composition was creamy. Observation of the silicone oil composition with a stereomicroscope revealed that the crosslinked silicone particles were uniformly dispersed in the silicone oil, and the shape of the crosslinked silicone particles was spherical.

Reference Example 7 A dimethylsiloxane-methylvinylsiloxane copolymer having a viscosity of 400 mPa · s and a dimethylvinylsiloxy group at both ends of the molecular chain (silicon-bonded vinyl group content = 1.18% by weight) 15.0 Parts by weight, viscosity 5
1.7 parts by weight of a dimethylsiloxane / methylhydrogensiloxane copolymer (content of silicon-bonded hydrogen atoms = 0.44% by weight) having a molecular chain of both ends capped at 0 mPa · s and trimethylsiloxy group, and a molecule having a viscosity of 20 mPa · s A crosslinkable silicone composition was prepared by mixing 83.3 parts by weight of dimethylpolysiloxane having trimethylsiloxy groups at both ends of the chain. Next, 3% by weight of polyoxyethylene nonyl phenyl ether (HLB = 13.0) was added to the crosslinkable silicone composition.
1) After adding 53 parts by weight of an aqueous solution and emulsifying by a colloid mill, 50 parts by weight of pure water was further added to prepare an aqueous emulsion of a crosslinkable silicone composition.

A separately prepared aqueous emulsion of a platinum-based catalyst containing 1,1-divinyl-1,1,3,3-tetramethoxydisiloxane complex of platinum as a main component (average particle diameter of platinum-based catalyst) = 0.05 μm, platinum metal concentration = 0.0
5% by weight) was added to the aqueous emulsion of the crosslinkable silicone composition described above in an amount such that the amount of platinum metal was 20 ppm by weight based on the dimethylpolysiloxane blocked with dimethylvinylsiloxy groups at both molecular chains in the emulsion. To form an aqueous emulsion of a crosslinkable silicone composition.

The emulsion is allowed to stand at room temperature for one day to perform a hydrosilylation crosslinking reaction of the crosslinkable silicone composition. This was prepared and used as a hair cosmetic raw material (G).

Next, the emulsion was transferred to an aluminum dish having a diameter of 5 cm and air-dried in a fume hood for 3 days to remove water, thereby preparing a silicone oil composition comprising silicone oil and crosslinked silicone particles. This silicone oil composition was creamy. Observation of the silicone oil composition with a stereomicroscope revealed that the crosslinked silicone particles were uniformly dispersed in the silicone oil, and the shape of the crosslinked silicone particles was spherical.

[Reference Example 8] 94.0 parts by weight of dimethylpolysiloxane blocked with dimethylvinylsiloxy groups at both ends of molecular chains having a viscosity of 400 mPa · s, and dimethylsiloxane methylhydrogen blocked with trimethylsiloxy groups at both ends of molecular chains having a viscosity of 30 mPa · s. 6.0 parts by weight of a siloxane copolymer (content of silicon-bonded hydrogen atoms = 0.5% by weight) was mixed to prepare a crosslinkable silicone composition. Next, 53 parts by weight of a 3% by weight aqueous solution of polyoxyethylene nonylphenyl ether (HLB = 13.1) was added to the crosslinkable silicone composition, and the mixture was emulsified by a colloid mill.
An aqueous emulsion of a crosslinkable silicone composition was prepared by adding 0 parts by weight.

A separately prepared aqueous emulsion of a platinum-based catalyst containing 1,1-divinyl-1,1,3,3-tetramethoxydisiloxane complex of platinum as a main component (average particle diameter of platinum-based catalyst) = 0.05 μm, platinum metal concentration = 0.0
5% by weight) was added to the aqueous emulsion of the crosslinkable silicone composition described above in an amount such that the amount of platinum metal was 20 ppm by weight based on the dimethylpolysiloxane blocked with dimethylvinylsiloxy groups at both molecular chains in the emulsion. To form an aqueous emulsion of a crosslinkable silicone composition.

The emulsion is allowed to stand at room temperature for one day to perform a hydrosilylation crosslinking reaction of the crosslinkable silicone composition to prepare an aqueous dispersion in which the crosslinked silicone particles are dispersed in water. (H).

Next, the emulsion was transferred to an aluminum dish having a diameter of 5 cm and air-dried in a fume hood for 3 days to remove water, whereby crosslinked silicone particles were obtained. When this was extracted with toluene and the extract was analyzed, the silicone oil content of the crosslinked silicone particles was 5% by weight or less.

Reference Example 9 A planetary mixer was charged with 44.5 parts by weight of a dimethylpolysiloxane having a vinyldimethylsiloxy group at both ends of a molecular chain having a viscosity of 5 mPa · s and a viscosity of 20 mPa.
100% by weight of methylhydrogenpolysiloxane (content of silicon-bonded hydrogen atoms = 1.5% by weight) having a molecular chain at both ends of a molecular chain of s, and a dimethyl having a molecular chain at both ends of a trimethylsiloxy group having a viscosity of 6 mPa · s. After mixing 758 parts by weight of the polysiloxane, 0.5 parts by weight of a 2% by weight solution of chloroplatinic acid in isopanol was added thereto to prepare a crosslinkable silicone composition. By stirring this crosslinkable silicone composition for 2 hours while heating it to 70 to 80 ° C., a hydrosilylation crosslinking reaction of the crosslinkable silicone composition was performed to prepare a soft silicone composition. This silicone oil composition was kneaded under shearing force with three rolls to prepare a paste-like silicone oil composition. This was designated as hair cosmetic raw material (I). Observation of the silicone oil composition with a stereomicroscope revealed that irregularly-shaped crosslinked silicone particles were dispersed in the silicone oil, but the dispersion was uneven, and the particle size of the crosslinked silicone particles was about 100 to 500 μm. It turned out to be big.

Reference Example 10 360 parts by weight of a polydimethylsiloxane capped at both ends of a molecular chain with a viscosity of 1,000,000 mPa · s and trimethylsiloxy groups capped at both ends of a molecular chain with a viscosity of 20 mPa · s 2
40 parts by weight were uniformly mixed, and 15 parts by weight of polyoxyethylene lauryl ether (HLB: 10.5) and 3 parts by weight of polyoxyethylene lauryl ether (HLB: 16.7) 3 were added thereto.
After 5 parts by weight and 40 parts by weight of pure water were added and emulsified, 310 parts by weight of pure water was further added to prepare a silicone oil emulsion, which was used as a hair cosmetic raw material (J).

[0095]

[Table 7]

[Examples 7 to 9 and Comparative Examples 6 and 7] Using the hair cosmetic raw materials (E), (F), (G), (H) and (J) prepared in the reference example, Table 8 was used. A shampoo of the indicated composition was prepared. Hair was washed using this shampoo, and the improvement in feel after washing and the improvement in combability were evaluated as follows. The results are shown in Table 8. [Evaluation Method for Improving Feeling of Hair] 10 g of a hair bundle having a length of 20 cm was washed with a 2.5% by weight aqueous solution of sodium polyoxyethylene lauryl ether sulfate, rinsed with warm water, and heated at 25 ° C.
, And pre-treated the hair. The pretreated hair was immersed in water for 30 seconds, drained, washed with 1 g of shampoo for 1 minute, rinsed with warm water twice for 20 seconds, drained, and the feel was evaluated. Then, it was dried under the condition of 25 ° C. for 12 hours,
The feel was evaluated. [Evaluation method for improving hair combability] 10 g of a hair bundle having a length of 20 cm was washed with a 2.5% by weight aqueous solution of sodium polyoxyethylene ether sulfate, rinsed with warm water, and heated at 25 ° C.
For 12 hours. This was immersed in water for 30 seconds, wrapped with a towel, drained under a pressure of 20 kgf / 314 cm ² for 5 seconds, and brushed until no catch was found, to perform hair pretreatment. The pretreated hair was washed with 1 g of shampoo for 1 minute, rinsed with warm water twice for 20 seconds, and then wrapped with a towel at 20 kgf / 314 cm ^2.
For 5 seconds and brushed until no longer caught. Next, the comb was set on the moving table using a tensile tester manufactured by Tester Sangyo Co., and one end of the treated hair was fixed, and this hair bundle was passed through the comb of the moving table.
The maximum value of the tensile force when the moving table was moved at 200 mm / min was measured. In addition, this was measured for each of the hair only subjected to the pre-treatment and the hair after the shampoo treatment, and the combing property improvement rate was determined by the following formula. Combability improvement rate (%) = 100 × (A−B) / A A = tensile force of hair pretreated only B = tensile force of shampooed hair

Comparative Example 8 A shampoo was prepared in the same manner as in Example 5 except that the hair cosmetic raw material (E) was used instead of the hair cosmetic raw material (E). Of the aggregated particles (100-20
0 μm), and a uniform shampoo could not be prepared.

[0098]

[Table 8]

Example 10, Comparative Examples 9 and 10 Hair cosmetic raw materials (E) and (H) were each 2% by weight and purified water 9
8% by weight was mixed to prepare a rinse. Using this rinse, the feel of the hair to the fingers and the amount of the crosslinked silicone particles attached to the treated hair were evaluated as follows, and the results are shown in Table 3.
It was shown to. Further, as a comparative example, a rinse in which purified water was increased in place of the hair cosmetic raw material (E) was prepared and similarly evaluated. The results are shown in Table 9. [Feeling of finger of hair] 10 g of a hair bundle of 20 cm in length was added to 2.
After washing with a 5% by weight aqueous solution of sodium polyoxyethylene lauryl ether sulfate, the hair was pre-treated by rinsing with warm water and drying at 25 ° C. for 12 hours. next,
After immersing the hair bundles in the above-mentioned rinses,
The hair was treated by drying at 5 ° C. for 12 hours. The slip and smoothness of the hair were evaluated as follows. ：: Very good ：: Good △: Neither of them ×: Poor [Amount of crosslinked silicone particles attached to hair] The rinsed hair was observed with an electron microscope, and the crosslinked silicone attached to the hair in a length of 100 μm. The number of particles was counted by observing the side of the hair from only one side.

[0100]

[Table 9]

Next, the average particle size and stability of the organic oil emulsion, the average particle size of the crosslinked silicone particles, and the characteristics of the organic oil composition were determined as follows. [Average Particle Size of Organic Oil Emulsion] The organic oil emulsion was measured with a laser diffraction type particle size distribution analyzer (LA-500 manufactured by HORIBA, Ltd.), and the obtained median diameter (particle size corresponding to 50% of the cumulative distribution) was measured. The average particle size was used. [Stability of Organic Oil Emulsion] A 225 mL glass bottle (105 mm deep,
(50 mm in diameter) and left at room temperature for 1 week. After standing, the thickness of the aqueous layer separated from the organic oil emulsion was measured. [Dispersibility of Crosslinked Silicone Particles] The organic oil emulsion was air-dried on a glass plate, and the shape, aggregation state, and distribution of the crosslinked silicone particles were observed under a stereoscopic microscope.
When all the crosslinked silicone particles were dispersed as primary particles, it was evaluated as ○. When there were aggregated particles of several hundred μm or primary particles of 500 μm or more, it was evaluated as ×, and between them was evaluated as Δ. [Average Particle Size of Crosslinked Silicone Particles] The organic oil emulsion was air-dried on a glass plate, and a crosslinked silicone particle was collected under a stereoscopic microscope to prepare a sample. The average particle size was determined from the above. [Viscoelasticity of Organic Oil Composition] About 10 g of an organic oil emulsion was placed in an aluminum dish, air-dried at room temperature for one week, and the storage elastic modulus G ′ (× 10 ³ d) of the organic oil composition from which water had been removed was obtained.
yne / cm ² ), loss modulus G '' (× 10 ³ dyne / cm ² ), loss tangent tan δ and complex viscosity (η *)
(Manufactured by Reometric Scientific). The measurement conditions were room temperature, 25 mm parallel plate, gap: 0.5 to 0.6 mm, and strain: 10
%, Frequency: 0.1 to 50 rad / s.

[Preparation of Cosmetic Raw Materials] Cosmetic raw materials were prepared as follows. Table 10 shows the properties of the cosmetic raw materials. [Reference Example 11] 9.01 parts by weight of a dimethylsiloxane-methylvinylsiloxane copolymer (containing silicon-bonded vinyl groups = 1.18% by weight) having a dimethylvinylsiloxy group at both ends of a molecular chain having a viscosity of 400 mPa · s. Trimethylsiloxy group-terminated dimethylsiloxane / methylhydrogensiloxane copolymer having a viscosity of 50 mPa · s at both ends of the molecular chain (content of silicon-bonded hydrogen atoms = 0.44% by weight) 0.99
Parts, isoparaffin (Nippon Petrochemicals Co. Isosol 400K, C ₁₆ H ₃₄₎ 85 parts by weight, viscosity 10 million
A crosslinkable silicone composition was prepared by mixing 5 parts by weight of dimethylpolysiloxane having a mPa · s molecular chain at both ends of a trimethylsiloxy group. Next, 30 parts by weight of a 3% by weight aqueous solution of polyoxyethylene nonylphenyl ether (HLB = 13.1) was added to the crosslinkable silicone composition, and the mixture was emulsified by a colloid mill. A water-based emulsion of an organic oil containing a water-soluble silicone composition was prepared.

A separately prepared aqueous emulsion of a platinum-based catalyst containing 1,1-divinyl-1,1,3,3-tetramethoxydisiloxane complex of platinum as a main component (average particle size of the platinum-based catalyst) = 0.05 μm, platinum metal concentration = 0.0
5 wt.
(About 1 part by weight) was uniformly mixed to obtain an aqueous emulsion of an organic oil containing a crosslinkable silicone composition.

The emulsion is allowed to stand at room temperature for one day to perform a hydrosilylation crosslinking reaction of the crosslinkable silicone composition, and the organic oil containing the crosslinked silicone particles in the organic oil droplets dispersed in water. An emulsion was prepared and used as a cosmetic raw material (K).

Next, this emulsion was transferred to an aluminum dish having a diameter of 5 cm and air-dried in a fume hood for one week to remove water, thereby obtaining a creamy organic oil composition. Observation of this organic oil composition with a stereomicroscope confirmed that the crosslinked silicone particles were uniformly dispersed in isoparaffin and high-viscosity silicone oil, and that the shape of the crosslinked silicone particles was spherical.

[Reference Example 12] A dimethylsiloxane-methylvinylsiloxane copolymer having a dimethylvinylsiloxy group at both ends of a molecular chain having a viscosity of 400 mPa · s (content of silicon-bonded vinyl group = 1.18% by weight) 22.0 8.0 parts by weight of a dimethylsiloxane-methylhydrogensiloxane copolymer (content of silicon-bonded hydrogen atoms = 0.05% by weight) having a trimethylsiloxy group at both ends of a molecular chain having a viscosity of 75 mPa · s and isoparaffin ( Nippon Petrochemicals Co. Isosol 400 K, and the C ₁₆ H ₃₄₎ 80 parts by weight with crosslinkable silicone composition was prepared. Then, 3% by weight of an aqueous solution of polyoxyethylene nonylphenyl ether (HLB = 13.1) was added to the crosslinkable silicone composition.
After adding 0 parts by weight and emulsifying with a colloid mill, 25 parts by weight of pure water was further added to prepare an aqueous emulsion of an organic oil containing a crosslinkable silicone composition. Reference Example 11
Prepare an organic oil emulsion in the same manner as above. This organic oil emulsion was used as a cosmetic raw material (L).

Next, this emulsion was transferred to an aluminum dish having a diameter of 5 cm and air-dried in a fume hood for 1 week to remove water, thereby obtaining a creamy organic oil composition. Observation of this organic oil composition with a stereomicroscope confirmed that the crosslinked silicone particles were uniformly dispersed in isoparaffin, and that the crosslinked silicone particles were spherical in shape.

[Reference Example 13] Crosslinked silicone particles (Toray
Dow Corning Silicone Trefil E-50
6, average particle size = 4 µm) 15 parts by weight and isoparaffin (Nippon Petrochemical Co., Ltd., Isosol 400K, C ₁₆ H ₃₄ ) 8
5 parts by weight were stirred and mixed to prepare a thixotropic organic oil composition in the form of a paste. To this organic oil composition, 53 parts by weight of a 3% by weight aqueous solution of polyoxyethylene nonylphenyl ether (HLB = 13.1) was added.
Further, 50 parts by weight of pure water was added to prepare an organic oil emulsion. This emulsion was used as a cosmetic raw material (M). Crosslinked silicone particles swollen with isoparaffin are aggregated on the surface of this organic oil emulsion,
It was uneven.

[Reference Example 14] 360 parts by weight of a dimethylpolysiloxane capped at both ends of a molecular chain having a viscosity of 1,000,000 mPa · s and 360 parts by weight of a dimethylpolysiloxane capped at both ends of a molecular chain having a viscosity of 20 mPa · s. Mix uniformly, add 15 parts by weight of polyoxyethylene lauryl ether (HLB = 10.5), 35 parts by weight of polyoxyethylene lauryl ether (HLB = 16.7) and 40 parts by weight of water, and mix. More water 31
0 parts by weight were added and mixed to prepare a silicone oil emulsion. This silicone oil emulsion was used as a cosmetic raw material (N).

[0110]

[Table 10] In addition, in Reference Example 13, the crosslinked silicone particles were aggregated particles (the primary particle size was 4 μm).

[Examples 11 and 12, Comparative Example 11] Table 11
3 with a homodisper at 2500 rpm
After stirring for minutes, an emulsion skin cosmetic was prepared. The skin cosmetics were evaluated as follows, and the results are shown in Table 11. [Feeling of skin cosmetics to fingers] A panel was asked to use cosmetics by 10 panelists, and the number of people who felt that the skin cosmetics felt good was 8 to 10 people, and 4 to 7 people. The case was evaluated as △, and the case of three or less was evaluated as ×. [Feeling of skin cosmetics on skin] 10 panelists used cosmetics and 8 to 10 people felt that the skin cosmetics had a good feeling, and 4 to 7 people The case was evaluated as △, and the case of three or less was evaluated as ×. [Dispersion state of crosslinked silicone particles in skin cosmetics] The skin cosmetics are thinly applied on a glass plate, and the particle diameter of the crosslinked silicone particles in the skin cosmetics is observed by an optical microscope, and the particle diameter is 10 μm or less. The dispersibility of the crosslinked silicone particles in the skin cosmetic was evaluated by determining the ratio of the crosslinked silicone particles exceeding 10 μm and the ratio of the crosslinked silicone particles exceeding 50 μm and the ratio of the crosslinking silicone particles exceeding 50 μm, respectively.

[0112]

[Table 11]

[Examples 13 and 14, Comparative Example 12] Table 12
A shampoo was prepared with the composition shown in Table 1. This shampoo was evaluated as follows, and the results are shown in Table 12. [Evaluation Method for Improving Feeling of Hair] 10 g of a hair bundle having a length of 20 cm was washed with a 2.5% by weight aqueous solution of sodium polyoxyethylene lauryl ether sulfate, rinsed with warm water, and heated at 25 ° C.
, And pre-treated the hair. The pretreated hair was immersed in water for 30 seconds, drained, washed with 1 g of shampoo for 1 minute, rinsed with warm water twice for 20 seconds, drained, and the feel was evaluated. Then, it was dried under the condition of 25 ° C. for 12 hours,
The feel was evaluated. [Evaluation method for improving hair combability] 10 g of a hair bundle having a length of 20 cm was washed with a 2.5% by weight aqueous solution of sodium polyoxyethylene ether sulfate, rinsed with warm water, and heated at 25 ° C.
For 12 hours. This was immersed in water for 30 seconds, wrapped with a towel, drained under a pressure of 20 kgf / 314 cm ² for 5 seconds, and brushed until no catch was found, to perform hair pretreatment. The pretreated hair was washed with 1 g of shampoo for 1 minute, rinsed with warm water twice for 20 seconds, and then wrapped with a towel at 20 kgf / 314 cm ^2.
For 5 seconds and brushed until no longer caught. Next, the comb was set on the moving table using a tensile tester manufactured by Tester Sangyo Co., and one end of the treated hair was fixed, and this hair bundle was passed through the comb of the moving table.
The maximum value of the tensile force when the moving table was moved at 200 mm / min was measured. In addition, this was measured for each of the hair only subjected to the pre-treatment and the hair after the shampoo treatment, and the combing property improvement rate was determined by the following formula. Combability improvement rate (%) = 100 × (A−B) / A A = tensile force of hair pretreated only B = tensile force of shampooed hair

[0114]

[Table 12]

[Comparative Example 13] A shampoo was prepared in the same manner as in Example 13 except that the cosmetic raw material (M) was used instead of the cosmetic raw material (K).
The dispersibility of (M) was poor, aggregated particles (100 to 200 μm) were generated, and a uniform shampoo could not be prepared.

[0116]

The cosmetic raw material of the present invention is characterized in that silicone oil or organic oil and crosslinked silicone particles can be uniformly dispersed in cosmetics. Further, the cosmetic of the present invention is composed of this cosmetic raw material and other cosmetic raw materials, in which silicone oil or organic oil and cross-linked silicone particles are uniformly dispersed, and the touch, elongation, and feeling on use to fingers and skin are improved. It has good characteristics, and it has characteristics that it can prevent fly hairs, floating hairs, tangles and entanglements, make hair easy to be tied up, and can give a dry feeling without stickiness. Furthermore, the method for producing cosmetics of the present invention is characterized in that such cosmetics can be efficiently produced.

──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat ゛ (Reference) A61K 7/06 A61K 7/06 7/075 7/075 (72) Inventor Ryuji Tachibana Chigusa Coast, Ichihara City, Chiba Prefecture 2-2 Toray Dow Corning Silicone Co., Ltd. Research and Development Headquarters (72) Inventor Tadashi Hamachi 2-2 Toray Dow Corning Silicone Co., Ltd. Research and Development Headquarters (72) Inventor Ozaki Katsu 2-2 Chikusa Beach, Ichihara City, Chiba Prefecture Toray Dow Corning Silicone Co., Ltd. Research and Development Division F-term (reference) 4C083 AA082 AB232 AB242 AB432 AC012 AC022 AC102 AC122 AC182 AC342 AC432 AC442 AC782 AD151 AD152 AD162 AD172 AD512 BB13 CC01 CC02 CC12 CC31 CC38 DD31 EE06 EE07 FF01 FF05 4J002 AE053 CH053 CP031 CP042 EA016 EH036 FD023 FD026 GB0 0

Claims (14)

[Claims] An average particle size of 0.1 to 5 dispersed in water.
Crosslinked silicone particles having an average particle size of 0.05 to 100 μm in droplets of 00 μm silicone oil or organic oil (however, the particle size of the crosslinked silicone particles is smaller than the particle size of the droplets of silicone oil or organic oil). Cosmetic raw material consisting of an emulsion of silicone oil or organic oil containing 2. Silicon oil or organic oil 2
The cosmetic raw material according to claim 1, wherein the viscosity at 5 ° C is 1 to 100,000,000 mPa · s. 3. The cosmetic raw material according to claim 1, wherein the crosslinked silicone particles have been subjected to a hydrosilylation crosslinking reaction or a condensation crosslinking reaction. 4. A crosslinkable silicone composition containing a non-crosslinkable silicone oil or an organic oil, wherein the silicone oil or the organic oil emulsion comprises a non-crosslinkable silicone oil or an organic oil.
The content of the non-crosslinkable silicone oil or organic oil is an amount exceeding the amount that the crosslinked product of the crosslinkable silicone composition can hold the non-crosslinkable silicone oil or organic oil. The cosmetic raw material according to claim 1, characterized in that (i) is dispersed in water and subjected to a crosslinking reaction. 5. A non-crosslinkable silicone oil or organic oil having a viscosity at 25 ° C. of from 1 to 100,000,000.
5. The cosmetic raw material according to claim 4, wherein the cosmetic raw material has a pressure of 0 mPa · s. 6. The cosmetic raw material according to claim 4, wherein the crosslinkable silicone composition is of a hydrosilylation crosslinking reaction type or a condensation crosslinking reaction type. 7. The cosmetic raw material according to claim 1, which is a skin cosmetic raw material. 8. The cosmetic raw material according to claim 1, which is a hair cosmetic raw material. 9. An oil composition in which crosslinked silicone particles are dispersed in a silicone oil or an organic oil obtained by removing water from the emulsion according to any one of claims 1 to 6. And cosmetic ingredients. 10. A cosmetic comprising the cosmetic raw material according to any one of claims 1 to 6 and another cosmetic raw material. 11. A skin cosmetic product,
The cosmetic according to claim 10. 12. It is a hair cosmetic,
The cosmetic according to claim 10. 13. A cosmetic comprising the cosmetic raw material according to claim 9 and another cosmetic raw material. 14. A method for producing a cosmetic, comprising mixing the cosmetic raw material according to claim 1 with another cosmetic raw material.